Process of obtaining vitamin-containing oils



' umj-guf S TES-PATENT OFFICE v l a tentedfiovils, r i f i I I PROCESSOF OBTAINING VITAMIN-CON TAINING OILS Ferdinand H. Young, Lake Blufl',and Hugh D. Robinson, North Chicago, Ill., assignors to AbbottLaboratories, North Chicago, 111., a. cornotation of Illinois NoDrawing. Application May 22, 1933, j

- Serial No. 672,344

'7: Claims. "(01; 87-6) The invention relates to a vitamin preparationThe temperature isthereupon increased by inparticularly useful for itsvitamin A. content and troduction of more live steam until a temperatoa; process for obtaining the same. f ture of 90 C. is reached. The massis stirred One ofthe primary objects of this invention is during theheating process which is maintained toprovide a product possessing a'substantially for about an hour. The stirring is then inter- 5 highervitamin A content than good medicinal rupted and the mass allowed tostand in the cod liver oil. Another object is to provide such tank forat least two hours, at the end of which a a product in the-form of a.stable, palatable and time the oil in the form of a semi-emulsion willefficacious liquid product substantially free from have separated andbe'floating on the surface.

10 disagreeable taste, odor, discoloring, and s'uh- The aqueous portionis drawn from beneath the W stantially free from many objectionableimpurioil and the emulsion placed in a suitable conties-such as fattyacids and nitrogenous bodies. tainer for further treatment to breaktheemm- A further .objectis to make available as a. 'sion and separatethe oil. commercial commodity a liquid vitaminprepara- Anysuitablemethod of removing the oil vfrom tion of such potency as to heeiiectivein dosages the emulsion may be employed, but preferably 15 measured indrops rather than in the standards this comprises the addition of threevolumes of such as teaspooniuls commonly used heretofore. a five percent saline solution. This is mixed Another object is to provide aprocess for ohintimately by stirring for fifteen minutes and tamingproducts as'ahove descrihed adapted for allowed to stand for two hours.Tins-partially at operation on a large commercial scale while inbreaksthe emulsion and washes the same free suringhigh purity of the Ldnaiproduct. "irom allrali. The washing is preferably repeated While theprocess is, in its broader aspects, a second time. The oil is thenheated by steam adaptable for the extraction of vitamimhearing to atemperature of 75 C. and placed in a oentricoils or fats from variousanimal or vegetable iuge capable of revolving at high speeds (iiillii asproducts, it is particularly adaptahle for ex- RP. MJ. The oil removedfrom the centrifuge tracting the vitamin content from. fish livers stillcontains traces of moisture and is somewhat and likeproducts. It alsofinds its greatest hazy. ;'l"'o eliminate the moisture, the oil isplaced utility in the preparation oi a high vitamin .in a tankands-suitable dehydrating agent added, oil from halibutlivers. Thereforewe will first such as anhydrous sodium sulphate. Agitation to describethe'process in its preferred form When is'continued. for a period oftwelve hours by suitusedin extracting halibut livers. a'ole means Whilethe oil is suitably protected The halibut livers when removed from theihh from oxidation. The preferred method for agimust he kept fresh bymaintaining them at a. tation consists in introducing a current ofcarbon low temperature, but they are preferably not-suhdioxide into thetank. A small quantity of illiterjected to a freezing temperature. Thefirst step ing medium, such as a special grade of iniusorial 555 theprocess is to-place the fresh halibut livers earth, may he added. andthe mixture passed in a tank containing Water at suficient temperthrougha. fllterpress, thereby obtaining an oilature to causejdisintegration ofthe levers with in-a. clear form ready for medicinal use. thecoagulation of the proteins. In the pre- The product obtained by theabove process is to ierredprocess the livers are placedin a. tank lightin color, substantially ireeirom disagreeto which is added hot water at82 C. The temable odor or. taste, contains less than one per perature ofthe water is lowered by contact cent of free fatty acids, and less thanone-tenth Withthe, cool livers but it is again brought up of one percent of nitrogenous material. The to the required degree by injectinglive steam product is golden yellow to amber in color and Whilethoroughly ring. Preferably the steam .has very little fishy odor ortaste. 'lheproduct Q5 is introduced until the temperature reaches 35? C.is highly potent since it contains not less than At this point there isadded suficient alkali such, 32,000 U. S. P. X. vitamin A units per gramof for example, as sodium hydroxide to neutralize oil as compared withstand d liver Oil which the free fatty acids. The exact amount of alkalihas but 400 such units per gram. The product added depends somewhat uponthe chemical also contains at least 2,008 A. D. M. Aritamln analysis ofthe halibut livers used, and-in some 1) units per gram as compared withstanda instances one per cent alkali is suificientl In cod liver oilwhich has only 100 such units D general, however, it will be foundsatisfactory gram. The product is adapted for oral adminis to add alkaliin an amount equivalent to two .tration and is.ofs11ch high potency thata suf- 5 and one-half per cent of the weight oithe livers. flcient'dailydose for ordinary purposes amounts to but a few drops of the liquid. itshould also be noted that while the minimum vitamin potency has beenindicated above, it is usual to obtain oil by means of our process whichhas a very much greater potency. In some cases the potency is as high as300,000 U. S, P. X vitamin A units per gram. The vitamin D potency doesnot usually increase at the same rate as the vitamin A potency and itdoes not in ordinary cases exceed 6,000 A. D, M. A; vitamin D units pergram.

It is to be understood that while our process has referred specificallyto certain preferred temperatures, the invention may be carried out attemperatures differing quite widely from those set forth. For example,it is possible to obtain an extraction at low temperatures bylengthening the, time of exposure to the alkali. On the other hand, thetemperature may in some instances be increased even above the boilingpoint. It is also to be noted that the use of saline in facilitating thebreaking of emulsions is not essential especially where a very highspeed centrifuge is used, or where a prolonged time for the separationmay be allowed.

While we have given examples of the preferred embodiments of ourinvention, it is to be understood that various modifications may be madewithout departing from the spirit of the invention, and we therefore donot-wish to be limited to the specific details of the processes exceptas indicated by the claims appended hereto.

What we claim as our invention is:

1. The process'of extracting livers containing oils rich in vitamins Aand/or D comprising treating said livers with a water solution, addingcaustic alkali in amount sufficient to liberate the oil from the solidbut insuflicient to cause a substantial amount of saponiilcation,causing an emulsion to separate from an aqueous solution and treatingsaid emulsion to remove therefrom an oil high in vitamins A and/or D andcontaining substantial amounts of saponifiable oil.

2. The process of extracting halibut liver comprlsingtreating thehalibut liver with a water solution, adding caustic alkali in amountsuificient to break up the cell tissue and liberate the oil butinsumcient to cause a substantially complete.

saponification of the oil, causing an emulsion to separate from anaqueous solution and treating said emulsion to remove therefrom an oilhigh in vitamins A and D and containing substantial amounts ofsaponifiable oil. 0

3. The process of extracting vitamin-containing oils or fats from fishproducts comprising treating the solid fish products with a watersolution at a high temperature not substantially above the boiling pointwhile maintaining a rapid agitation, adding caustic alkali in amountsufficient to break up the cell tissue and liberate the oil but in:lificient to cause a substantially complete saponification of the oil,allowing the mass to stand until an emulsion separates from an aqueoussolution and treating the emulsion to remove therefrom an oil high invitamin content and containing substantial amounts of saponifiable oil.

4. The process of obtaining a highly purified high potency halibut liveroil comprising adding water to fresh halibut levers, maintaining thewater at a high temperature not substantially above the boiling pointthereof, adding an alkali metal hydroxide in quantity sufllcient tosubstantially neutralize the free fatty acids, break up the cell tissueand liberate the oil but in'suflicient to cause a substantially completesaponification of the oil agitating the mass, allowing the mass to fromsaid emulsion, thereby obtaining an oil high,

in vitamins A and/or D and containing substantial amounts ofsaponifiable oil.

6. The process of extracting livers containing oils rich in vitamins Aand/or D comprising adding waterto said livers, adding suflicientcaustic alkali to substantially neutralize the fatty acids andinsuflicient to cause a. substantially complete saponiilcation of oil,causing an emulsion to separate from an aqueous layer, adding a salinesolution to said emulsion, separating the oil from said emulsion andtreating the oil thus obtained with a dehydrating agent, therebyobtaining an oil in a clear form ready for medicinal use and containingsubstantial amounts of saponifiable oil.

' '7. The process of extracting a highly purified high potencyhalibut'liver oil comprising adding hot water to fresh halibut livers,injecting live steam into the mass until the temperature issubstantially 0., adding caustic soda in an amount equivalent toapproximately two and onehalf per cent alkali on the basis of the weightof the livers, introducing steam into the mass until a' temperature ofapproximately C. is reached, allowing the mass to stand until anemulsion separates from an aqueous layer, adding a saline solution tosaid emulsion, heating the oil obtained therefrom to a temperature ofapproximately 75 C. and subjecting the same to a high speed centrifuge,treating the oil from said centrifuge with anhydrous sodium sulphate,adding a filtering medium and filtering through a filter press to obtainan oil suitable for medicinal use and containing substantial amounts ofsaponifiable oil.

FERDINAND H. YOUNG. HUGH D. ROBINSON.

